Smoking product



United States Patent SMOKING PRODUCT Sheldon Rosenberg, Westport, andOtto Karl Schmidt, Springdale, Conn., assignors to International CigarMachinery Company, Inc., a corporation of New Jersey No Drawing. FiledSept. 9, 1959, Ser. No. 838,854

11 Claims. (Cl. 131-17) duce desired shades of color in smoking productsis well known. Several patents dislcose the use of vegetable dyes tocontrol the color of tobacco. Such dyes have also been used in preparingtobacco sheets from finely ground tobacco and adhesives of varioussorts.

Most useful dyes are water-soluble. Thus when in contact with salivafrom the smokers mouth dye tends to dissolve out of the tobacco productat a rate significantly greater than the natural pigments of tobacco.This results in an undesirable dark shade at the head end of the smokingarticle.

The use of water-insoluble pigments and dyes overcomes some of thesolubility problems. It has, however, been found that these productsoften have other objectionable qualities. For example,2-(2-quinolyl)-1-3- indandione (Drug and Cosmetic Yellow #11) althoughproducing good, colored tobacco products, has a tendency to sublime andproduce a yellow colored smoke. Use of iron oxide pigments, for example,results in reddish-yellow residues in the ash.

It has been known for some time in the dye industry that certainwater-soluble dyes may be laked onto inert carriers such as alumina andthereby be converted to water insoluble forms.

In the manufacture of tobacco it has been a common practice toincorporate ash and burn additives. A wide variety of such compounds asdiatomaceous earth, bentonite, asbestos, montmorillonite clays, kaolin,and silicious particle materials of various types, have been used forthis purpose.

It is an object of this invention to manufacture a smoking productcharacterized by the use of tobacco in combination with initially watersoluble dyes which have been laked onto inert carriers useful for ashand burn control.

Another object of this invention is to provide a tobacco product, suchas a sheet, in which tobacco is combined with an adhesive andreinforcing fibers upon which an initially water soluble dye has beenlaked to make the dye insoluble.

'and washed free of sulfate ions.

2,977,254 Patented Mar. 28, 1961 A further object of this invention isto form insoluble dyestuffs from water soluble dyes, readily combinedwith tobacco in aqueous systems commonly used in the manufacture oftobacco.

Contrary to the well known technique of laking on alumina, a superiorproduct may be obtained according to this invention by forming the lakeon a carrier which can later have double utility, namely to cause thedye to be uniformly distributed in an insoluble form and also to givecontrol over the texture and color of the ash when tobacco containingthe lake or lakes, is used either as wrapper or binder for cigars or asfiller for cigarettes.

In the following examples, IA-D and IIA-C illustrate how to preparepigment for'use in tobacco manufacture.

Example I-A Twenty gms. of aluminum sulfate were dissolver in 200 cc. ofhot water and 32 gms. of an amorphous diatomaceous earth was added. Themass was agitated for 15 minutes and cooled to room temperature. To theabove, gms. of aqueous 10% sodium carbonate solution was added slowly,stirred for 30 minutes, filtered,

The filter cake was resuspended in 200 cc. of water and 1.4 g. of thetrisodiurn salt of3-carboxy-5-hydroxy-l-p-sulfophenyl-4-p-sulfophenylazopyrazole (Food,Drug and Cosmetic [RD and C.], Yellow #5), dissolved in 100 cc. water,was added slowly to the suspended cake material. After 30 minutes a 10%solution of aluminum chloride was added in small quantities up to atotal of 5-9 cc. while titrating tests were made after each addition todetermine when the dye was fixed. The color is usually fixed when the pHof the charge is lowered to 5.5 by sufiicient amounts of aluminumchloride.

After complete fixation of the color the batch was stirred gently for 30minutes and then filtered. The filter cake was washed twice with 100 cc.water in a filtered device to form a dye preparation. The pigment can beused in its wet form with tobacco.

Example I-B The base was prepared as in Example I-A. The FD. and C.Yellow #5 was replaced by the disodium salt of1-pseudocumylazo-2-naphthol-3-6-disulfonic acid (RD. and C. Red #1). Apigment resulted which was of bright red color with very good fixationcharacteristics and fastness.

Example I-C The base Was prepared as in Example I-A. The PD. and C.Yellow #5 was replaced by the trisodium salt of1-(4-sulfo-l-naphthylazo)-2-naphthol-3,6 disulfonic acid (RD. and C. Red#2). A pigment resulted which was of bluish-red color and had good bleedresistance and fair fixation characteristics.

Example l -D mixing continued for 30 minutes. A homogeneous uniformlycolored filter cake was obtained. This was washed twice with 100 cc.water. The product was comparable in tinctorial power to material madeaccording to Example I-A.

In addition to diatomaceous earth, the dyes shown above can be laked outon bentonite, silica gel, kaolin, and other inorganic carriers. Theresulting products are similar to the diatomaceous earth lakes butresult in some difierences in properties of tobacco products. Forexample, the bentonite lakes produce an extremely coherent, non flakingash which is a desirable characteristic for cigars.

Additional water insolubility and bleed resistance of these lakes can beachieved through the use of rosin sizings in the lake preparation.

In addition to the process described above, the lake may also beprepared in such a way that the color is adsorbed on cellulose fiberswhich can be used for reinforcing tobacco films. The following areexamples of this technique.

Example IIA A pulp consisting of pounds of refined cellulose fibers,which may be from tobacco, in 200 pounds of water was treated with onepound of a 1% by weight solution of ED. and C. Yellow #5. To thesuspension The procedures shown in Example IIA were followed with theexception that the dye was the disodium salt of 4-[ [4-(N-ethyl-p-sulfobenzyl amino) phenyl] (4-sulfoniumphenyD-rnethylcne][1-(N-ethyl-N-p-sulfobenzyl)- 13 cyclohexadienimine], (ED. and C. Green#2). The product was color fast and non-bleeding. A test sheet made fromthe fibers had excellent tensile properties and good color stabilitywhen wet.

Example I1-C The process of Example II-A was carried out, except thatthe dye was the disodium salt of 5,5-indigotin disulfonic acid (ED. andC. Blue #2).

The above lakes were used in manufacturing tobacco by processesillustrated below in Examples IIIV. Such tobacco may be used for wrapperon cigars, cigarillos, or little cigars, as binder for cigars, or asfiller for cigars, cigarettes, or pipe tobacco.

Example 111 The process for laking ED. and C. Yellow #5 on diatomaceousearth shown in Example I-A was used to prepare 100 pounds of a wetfilter cake containing 35% solids. The dye content of the lake was 3.5%on a dry basis.

A tobacco product was prepared according to the process described inExample I of US. Patent 2,887,414. The proportion of ingredients wasidentical except that 12 pounds of the 35% diatomaceous earth lake ofYellow #5 was added to the dispersion.

The resulting tobacco product was light tan in color as opposed to thedeep brown of the control sheet. No noticeable differences in strengthproperties were found, but it was observed that the ashproduced whenthis product was used as a binder on cigars, was extremely coherent andlight grey. Smoking quality was judged by a panel of experts to besuperior to the untreated control cigar.

4! Example I V-A The green dyed fibers of Example II-B were used'toprepare a tobacco product in the following manner. The consistency ofthe fibers was adjusted to 2% by weight. A dry blend composed of onepound of carboxymethyl cellulose of a type having a 2% Brookfieldviscosity of between 200 and 500 centipoises, two pounds of groundmontmorillonite silicious catalyst, and 0.8 pound of polyglyoxal wasdispersed into 200 pounds of the 2% fiber dispersion. After completemixing, five pounds of tetraethylene glycol were added. To the resultingdispersion, 75 pounds of a 4% by weight solution of ethyl-hydroxyethylcellulose of a type which as a 2% Brookfield viscosity of 1100centipoises were added and mixed. The resulting adhesive solution wasadjusted to 5% solids, was then continually mixed with a total of 25pounds of tobacco powder which passed an 80 mesh screen to form a slurrywhile metering said slurry onto a continuous stainless steel belt with acasting knife. The thin uniform film was dried, remoistened, doctoredfrom the belt, rolled up, and slit into bobbins for use on a wrapperfeed device of cigar machines. The wrapper was somewhat greenish and hadthe appearance of a good Havana wrapper. Cigars made with this wrappershowed no discoloration at the heads, held up well on chewing, andsmoked well with a resultant light grey coherent ash.

Example IV-B The process of Example IV-A was used except that thebinding agent was locust bean gum and the fibers were derived fromtobacco stems. Essentially the same results were obtained.

Example V Samples of wrapper-type tobacco which had been spotted by thewell-known disease, weather-fleck, were treated by this invention. Ayellow pigment was prepared according to Example I-A.

One pound of the pigment was dispersed in a solution composed of 2 lbs.of ethyl cellulose in 98 lbs. of a solvent containing 3 parts by Weightof benzene and one part by weight of methyl alcohol. After completedispersion the pigment solution was sprayed on the wrapper leaves. Afterdrying the resulting leaves had a light golden cast and were improved inquality. Cigars wrapped with the treated leaves were uniform in colorand showed little or no evidence of the disease spots.

What is claimed is:

1. A smoking product comprising in combination an inert carrier, a watersoluble dye mordanted upon said inert carrier and tobacco.

2. A smoking product according to claim 1 in which the carrier isinorganic.

3. A smoking product according to claim 2 in which Y the carrier isselected from the group consisting of diatomaceous earth, silica gel,bentonite, asbestos, montmorillonite clay, kaolin, and siliciousparticles.

4. A smoking product according to claim 1 in which the laked dye isselected from the group consisting of:

Trisodium salt of 3-carboxy-5-hydroxy-1-p-sulophenyl-4-p-sulfophenylazopyrazole; disodium salt ofl-pseudocumylazo-2-naphthol-3-6-disulfonic acid; trisodium salt of1-(4-sulfo-1-naphthylazo)-2-naphthol-3,6 disulfonic acid; disodium saltof 4-[[4-(N-ethyl-p-sulfobenzyl amino) phenyl] (4-sulfoniumphenyl)methylene]- [1-(N-ethyl-N-p-sulfobenzyl) A cyclohexadienimine]; anddisodium salt of 5,5-indigotin disulfonic acid.

5. A smoking product according to claim 1 which includes rosin size.

6. A smoking product according to claim 1 in which the carrier iscellulosic fiber.

7. A smoking product comprising in combination tobacco, a dye and aninert inorganic material upon which has been mordanted said dye materialconsisting of Yellow #5.

8. A smoking product comprising tobacco, a water tobacco, a dye andcellulose fibers upon which has been soluble dye and a celluloseadhesive upon which has mordanted said dye material consisting of Green#2. been mordanted said water soluble dye.

9. A smoking product comprising in combination References Cited in thefile of this patent tobacco, a water soluble dye and dyed tobaccofibers- 5 upon which has been mordanted said water soluble dye. UNITEDSTATES PATENTS 10. A smoking product comprising in combination 1,756,778Alden Apr. 29, 1930 tobacco, a dye and cellulose fibers upon which hasbeen 1,863,813 Alden et a1 June 21, 1932 mordanted said dye materialconsisting of Yellow #5. 1,972,718 Sharlit Sept. 4, 1934 11. A smokingproduct comprising in combination 10

1. A SMOKING PRODUCT COMPRISING IN COMBINATION AN INERT CARRIER, A WATERSOLUBLE DYE MORDANTED UPON SAID INERT CARRIER AND TOBACCO.